WO2011034110A1 - 金属酸化物-金属複合スパッタリングターゲット - Google Patents
金属酸化物-金属複合スパッタリングターゲット Download PDFInfo
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- WO2011034110A1 WO2011034110A1 PCT/JP2010/065988 JP2010065988W WO2011034110A1 WO 2011034110 A1 WO2011034110 A1 WO 2011034110A1 JP 2010065988 W JP2010065988 W JP 2010065988W WO 2011034110 A1 WO2011034110 A1 WO 2011034110A1
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/26—Apparatus or processes specially adapted for the manufacture of record carriers
- G11B7/266—Sputtering or spin-coating layers
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
- G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
- G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
- G11B2007/24302—Metals or metalloids
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
- G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
- G11B7/243—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising inorganic materials only, e.g. ablative layers
- G11B2007/24318—Non-metallic elements
- G11B2007/2432—Oxygen
Definitions
- the present invention relates to a metal oxide-metal composite sputtering target useful for forming a recording layer for an optical information recording medium.
- the recording layer of an optical information recording medium such as Blu-ray Disc is composed of various materials such as an inorganic material and an organic material.
- a recording layer made of an inorganic material sputters a sputtering target of the same material as the recording layer. It is preferable to form by a sputtering method.
- the sputtering method means that a plasma discharge is formed between a substrate and a sputtering target in a sputtering chamber into which Ar is introduced after evacuation, and Ar ionized by the plasma discharge is made to collide with the sputtering target, In this method, atoms of the sputtering target are knocked out and deposited on a substrate to produce a thin film.
- In-plane uniformity of component composition and film thickness in the film surface direction (in the film surface) is smaller in the thin film formed by sputtering compared to thin films formed by ion plating, vacuum evaporation, and electron beam evaporation. Is excellent. Further, unlike the vacuum deposition method, the sputtering method has an advantage that a thin film having the same component composition as the sputtering target can be formed.
- Patent Document 1 discloses a write-once optical recording medium including a recording layer having a first reaction layer and a second reaction layer.
- a mixture of ZnS and SiO 2 is formed on a substrate.
- a second dielectric layer made of Cu, a second reaction layer made of Cu, a first reaction layer made of Si, and a first dielectric layer made of a mixture of ZnS and SiO 2 are sequentially formed by sputtering.
- details of the sputtering method are not described at all.
- Patent Document 2 discloses an optical information recording medium having a recording layer made of Te, O, and a predetermined element M.
- a Te—O—Pd recording layer was formed by sputtering. It is stated. However, the actual situation is that sputtering is performed using a Te—Pd target in an atmosphere of a mixed gas of Ar and O 2 , and a composite sputtering target containing a metal oxide and a metal is not disclosed.
- the present invention has been made in view of the above circumstances, and an object thereof is to provide a metal oxide-metal composite sputtering target useful for forming a recording layer for an optical information recording medium containing a metal oxide and a metal. There is.
- the present invention includes the following aspects.
- Metal oxide containing metal oxide A and metal B-metal composite sputtering target wherein the maximum equivalent circle diameter of the metal oxide A is controlled to 200 ⁇ m or less- Metal composite sputtering target.
- the metal oxide A may be aggregated.
- the metal oxide A is at least one selected from the group consisting of In oxide, Bi oxide, Zn oxide, W oxide, Sn oxide, Co oxide, Ge oxide, and Al oxide. 3) The metal oxide-metal composite sputtering target according to any one of 3). (5) The metal oxide according to any one of (1) to (4), wherein the metal B is at least one selected from the group consisting of Pd, Ag, W, Cu, Ge, Co, and Al. Metal composite sputtering target. (6) The metal oxide-metal composite sputtering target according to any one of (1) to (5), which is used for forming a recording layer for an optical information recording medium.
- the maximum value of the equivalent circle diameter of the metal oxide is controlled to 200 ⁇ m or less, so that abnormal discharge occurs during sputtering or cracking of the sputtering target due to thermal stress occurs.
- a metal oxide-metal composite recording layer corresponding to the composition of the sputtering target can be efficiently produced without causing the problem of occurrence.
- the relative density of the metal oxide-metal composite sputtering target of the present invention is preferably controlled to 92% or more, the operation can be performed without causing problems such as gas generation from the sputtering target during sputtering. stable, productivity is enhanced.
- FIG. 1 (a) and 1 (b) show the No. used in the examples. It is an optical microscope photograph showing the structure
- the present inventors have used a metal oxide-metal composite sputtering target (hereinafter sometimes simply referred to as a composite sputtering target) useful for forming a recording layer for an optical information recording medium containing a metal oxide and a metal.
- a composite sputtering target useful for forming a recording layer for an optical information recording medium containing a metal oxide and a metal.
- the metal oxide is easily aggregated, and the aggregated oxide (oxide aggregate phase) is poor in sinterability compared to the metal, so that defects tend to remain inside the oxide aggregate phase.
- the oxide aggregate phase is charged (charged up). Abnormal discharge may occur.
- the large oxide aggregate phase also becomes an impediment to heat conduction, and cracking of the sputtering target is likely to occur.
- a decrease in the relative density of the composite sputtering target causes a decrease in thermal conductivity and strength.
- the input power is set to be high for the purpose of improving productivity, the sputtering is performed.
- the temperature of the target surface (sputtering surface) rises, and thermal stress is generated due to the temperature difference between the front surface and the back surface. Since the metal oxide is a brittle material, the thermal stress easily causes cracks in the sputtering target. For this reason, the input power cannot be set high, resulting in a decrease in the film formation rate and, in turn, a decrease in productivity of the optical information recording medium.
- the present inventors can solve the above-mentioned problems associated with the coarsening of the metal oxide aggregated phase and, more preferably, the problems associated with the decrease in the relative density of the composite sputtering target.
- the type and mixing method of the mixer should be appropriate so that the raw material powder (metal oxide A and metal B) can be uniformly mixed, and even if the metal oxide A aggregates, there is no large aggregate phase.
- the maximum value of the equivalent circle diameter of the metal oxide A is 200 ⁇ m or less, preferably by relative sieving before mixing, if necessary.
- the present inventors have found that metal oxide-metal composite sputtering having a density controlled to 92% or more can be obtained.
- the sputtering target of the present invention is a composite sputtering target containing metal oxide A and metal B, and the maximum equivalent circle diameter of metal oxide A is controlled to 200 ⁇ m or less.
- the maximum equivalent circle diameter of the metal oxide A should be small, preferably 180 ⁇ m or less, more preferably 100 ⁇ m or less.
- the maximum value of the equivalent circle diameter of the metal oxide A is controlled to 200 ⁇ m or less” means that the metal oxide A may be aggregated (of course, it may not be aggregated). However, even when the metal oxide A aggregates to form an aggregated phase, it means that the circle equivalent diameter of the metal oxide A satisfies 200 ⁇ m or less at the maximum. Specifically, when the equivalent circle diameter of the metal oxide A in the observation visual field is measured by the following procedure, it is necessary that the maximum diameter satisfies 200 ⁇ m or less in any observation visual field.
- the reason why the “maximum value” (maximum diameter) is defined instead of the average value of the equivalent circle diameter of the metal oxide A is that even if the equivalent circle diameter of the metal oxide A is controlled to be small on average. This is because it has been proved by the basic experiments of the present inventors that the above-mentioned problems are caused when even one metal oxide A having a maximum diameter exceeding 200 ⁇ m exists in the observation field.
- a sputtering surface to be measured is prepared.
- the sputtering target is cut along a plane parallel to the sputtering surface to expose the sputtering surface to be measured.
- the measurement target is the vicinity of the sputtering target surface, preferably the cut surface of the target outermost surface.
- the sample cut as described above is embedded in a resin such as an epoxy resin, and the observation surface is mirror-polished.
- etching of the sputtering surface is unnecessary.
- the equivalent circle diameter of the metal oxide A contained in the surface of the sputtering surface after mirror polishing is observed with a microscope.
- Microscopic observation is performed using an optical microscope or a scanning electron microscope (Scanning Electron Microscope: SEM).
- SEM scanning Electron Microscope
- a plurality of locations can be arbitrarily selected as the selected portion of the sputtering surface, but more accurate selection of the maximum equivalent circle diameter of the metal oxide can be obtained by selecting as many as possible. In the present invention, for example, it is preferable to select about 5 to 9 locations per 30000 mm 2 of the sputtering surface.
- the magnification for microscopic observation may be appropriately set according to the equivalent circle diameter of the metal oxide A, but is usually set to about 100 to 200 times. For example, when it is determined whether or not the metal oxide A has an equivalent circle diameter exceeding 200 ⁇ m, it is preferable to set the magnification to about 100 times and increase the visual field area.
- the number of photomicrographs may be appropriately controlled according to the magnification. For example, when the magnification is set to about 100 times, it is preferable that the number of micrographs is set to three or more fields at random. On the other hand, when the magnification is set to about 200 times, it is preferable to further increase the number of fields of view. However, when a large aggregated phase of metal oxide A is not clearly observed during observation, it is sufficient to set the magnification to about 100 times, and the field of view may be randomly set to three or more fields.
- the equivalent circle diameter of the metal oxide A is measured by image analysis.
- Image analysis is performed using NanoHunter NS2K-Pro manufactured by Nano System Co., Ltd. Since the image analysis apparatus includes a program for automatically calculating all the above-described equivalent circle diameters, these are automatically obtained.
- the maximum value is 200 ⁇ m or less in any field of view.
- the relative density of the sputtering target of the present invention is preferably 92% or more.
- problems such as operation instability due to gas generation during sputtering and generation of cracks due to thermal stress can be solved.
- the relative density is a value measured by a normal Archimedes method.
- the sputtering target of the present invention is a composite sputtering target containing a metal oxide A and a metal B, and the maximum equivalent circle diameter of the metal oxide A and preferably the relative density is controlled as described above. Although all are included regardless of the composition, it is preferable to set the composition mainly considering the following (I) and (II).
- the sputtering target of the present invention is preferably used for forming a recording layer for an optical information recording medium, and the composition of the sputtering target so as to satisfy the main characteristics required for the recording layer. It is also desirable to be controlled. Specifically, for example, it must have sufficient reflectivity for reproducing recorded signals, be able to record with practical recording laser power (having high recording sensitivity), and have sufficient signal amplitude for reproducing recorded signals.
- the present invention provides a sputtering target useful for forming a recording layer for an optical information recording medium that satisfies required characteristics such as having (having a high degree of modulation) and having a high signal intensity (having a high C / N ratio). From the viewpoint, it is preferable to appropriately control the composition of the sputtering target.
- metal oxide A and metal B are preferably used in the presence of a solvent such as water.
- a solvent such as water.
- melting points such as In and Bi generally have a melting point as low as 500 ° C. or less dissolve when the sputtering target is manufactured (sintered)
- low melting point metals such as In and Bi are used as metal B. Is preferably used as the metal oxide A in the form of an oxide.
- a metal which is unstable in the form of a metal oxide such as Pd (PdO 2 decomposes at a temperature of about 700 ° C.) only as the metal B.
- some metals may be used as the metal oxide A or the metal B, such as W or Co. As shown in Examples described later, in the present invention, W and Co are used in any form.
- preferred metal oxides A and B constituting the sputtering target of the present invention are as follows.
- the metal oxide A is preferably at least one selected from the group consisting of In oxide, Bi oxide, Zn oxide, W oxide, Sn oxide, Co oxide, Ge oxide, and Al oxide. These may be contained independently and 2 or more types may be used together.
- the metal B is preferably at least one selected from the group consisting of Pd, Ag, W, Cu, Ge, Co, and Al. These may be contained independently and 2 or more types may be used together.
- examples of preferable combinations of the metal oxide A and the metal B include (a) Zn oxide + W + Pd and (b) oxide In + Pd.
- a method for producing the sputtering target of the present invention will be described.
- a mixing step of raw material powders (metal oxide A and metal B) is particularly suitable. It is extremely important to control it. Specifically, as described below, it is preferable to select a suitable mixing method according to the type of the mixer.
- the mixer used in the mixing step is a raw material powder such as a V-type mixer with stirring blades and a horizontal cylindrical mixer with internal blades. It is preferable to mix using a mixer having a shearing action. This is because the agglomerated portion (agglomerated phase) is crushed even if the metal oxide A is agglomerated by a stirring blade or an internal blade installed in the mixer, and thus aggregation of the raw material powder is suppressed.
- the method of mixing using the above mixer is not particularly limited, and the type, amount, and mixing of the raw material powder so that the maximum circle equivalent diameter of the metal oxide A does not exceed 200 ⁇ m. Depending on the type of machine, etc., it should be set appropriately.
- the mixing time is controlled in the range of 60 to 90 minutes
- the number of stirring is 30 to 70 rpm
- the internal blades are in the opposite direction to the cylinder. It is preferable to control in the range of 100 to 500 rpm.
- a mixer having no shearing action a normal mixer having no shearing action [V-type mixer (V mixer), horizontal cylindrical mixer, etc.] can also be used.
- V-type mixer V mixer
- horizontal cylindrical mixer etc.
- a sputtering target in which the maximum value of the circle-equivalent diameter of the object A is appropriately controlled can be obtained (see examples described later).
- a mill such as a ball mill or a vibration mill can be used as a mixer.
- the mill is usually used for crushing the raw material powder, but in the present invention, the mill can be used for crushing and mixing the raw material powder.
- under wet conditions means mixing in the presence of a solvent such as water.
- the mixing conditions are not particularly limited, and may be appropriately set according to the type and amount of the raw material powder, the type of mill, and the like so that the maximum equivalent circle diameter of the metal oxide A does not exceed 200 ⁇ m.
- raw material powder, alumina balls and water are put into a ball mill, mixed for a predetermined time, taken out, dried, and coarsely pulverized, preferably by pulverizing in a mortar. Then, it is preferable to use for a sintering process.
- Adjustment of particle size distribution before mixing for metal oxide A for the purpose of removing coarse powder before mixing and appropriately controlling the particle size distribution, it is passed through a sieve of a predetermined size. It is preferable to mix only those that have passed through.
- the above (2) is not necessarily an essential step, and it is preferable to carry out an appropriate combination depending on the type of the mixer.
- the above (2) may or may not be performed. In either case, the desired metal oxide A
- a sputtering target having the maximum value of the equivalent circle diameter has been confirmed in the examples described later.
- the mixing ratio of the metal oxide A and the metal B may be appropriately controlled in accordance with the desired composition of the recording layer for an optical information recording medium.
- the mixed powder obtained as described above is sintered.
- Examples of the sintering method include HIP (Hot Isostatic Pressing), hot pressing, and the like, but it is preferable to perform discharge plasma sintering described in Examples described later.
- the spark plasma sintering method is a method in which a DC pulse current is passed while pressing the mixed powder, and discharge plasma is generated between the powders to sinter. It can be sintered in a short time (several minutes) and handled. It has the advantage of being easy. Since the specific conditions of the spark plasma sintering method differ depending on the type and amount of the raw material powder, the heating temperature is determined in a preliminary experiment. Further, in order to increase the density, it is preferable that the applied pressure is high, and it is preferable to control the pressure within the range of 40 to 50 MPa.
- a sputtering target is manufactured by machining the sintered body obtained as described above.
- Examples of the machining method include machining using a lathe or a milling machine, but machining using an NC lathe described in Examples described later is preferable.
- a thin film formed by a sputtering method using the sputtering target thus obtained is particularly preferably used for a recording layer of an optical information recording medium.
- Example 1 Compound sputtering targets (No. 1 to 14) containing metal oxide A and metal B having various compositions shown in Table 1 are mixed by the method shown in Table 1, then sintered and machined to produce. did.
- oxidized In powder oxidized In made of rare metal, purity 99.9%, average particle size 7.3 ⁇ m, standard deviation SD 1.0 ⁇ m
- Pd powder Ishifuku Metal, average particle size 2.0 ⁇ m, Standard deviation SD 0.5 ⁇ m
- the oxidized In powder was used by removing coarse particles in advance using a 100 mesh sieve before mixing, and using only the powder that passed through the sieve.
- these raw material powders were put into a vibration mill and mixed under wet conditions. Specifically, an alumina ball having a diameter of 10 mm, 400 g of the above raw material powder (228 g of oxidized In powder, 172 g of Pd powder), and 800 mL of water were added to a vibration mill, and then mixed under the conditions shown in Table 1. Then, after drying at 140 degreeC for 2 hours, it crushed in the mortar, and what passed the 36 mesh sieve was used for the next sintering process.
- the sintering method was performed using a discharge plasma sintering machine (SPS-3.20MK-IV manufactured by Sumitomo Heavy Industries). Specifically, the mixed powder was filled in a graphite mold ⁇ 105 mm, placed in the sintering machine, and sintered at a heating temperature of 1000 ° C. and a pressing force of 50 MPa for 1 hour. Next, machining was performed with an NC lathe. 1 sputtering target was manufactured.
- SPS-3.20MK-IV manufactured by Sumitomo Heavy Industries
- these raw material powders were put into a mixer equipped with stirring blades (manufactured by Kobelco Research Institute in-house) and mixed. Specifically, 450 g of the above raw material powder (247.5 g of oxidized In powder, 157.5 g of Pd powder, and 45 g of Ag powder) was added to the above mixer, and then mixed under the conditions shown in Table 1. Used in the next sintering step.
- Sintering method is no. In the same manner as in No. 1, a spark plasma sintering machine was used, and sintering was performed at a heating temperature of 940 ° C. and a pressure of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. 3 sputtering targets were produced.
- these raw material powders were put into a ball mill and mixed under wet conditions. Specifically, a ⁇ 10 mm alumina ball, 500 g of the above raw material powder (325 g of oxidized In powder, 150 g of Pd powder, and 25 g of W powder) and 700 mL of water were added to a ball mill and mixed under the conditions shown in Table 1. did. Then, after drying at 140 degreeC for 2 hours, it crushed using the mortar, and what passed the 36 mesh sieve was used for the next sintering process.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 1000 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. 1 performs machining in the same manner as, No. 4 of the sputtering target was produced.
- these raw material powders were put into a ball mill and mixed under wet conditions. Specifically, after adding ⁇ 10 mm alumina balls, 500 g of the above raw material powder (275 g of Zn oxide powder, 25 g of oxidized W powder, and 200 g of Pd powder) and 700 mL of water in a ball mill, the conditions shown in Table 1 were applied. Mixed. Then, after drying at 140 degreeC for 2 hours, it crushed using the mortar, and what passed the 36 mesh sieve was used for the next sintering process.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 950 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. 1 performs machining in the same manner as, No. 5 sputtering target was produced.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 1000 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. 6 sputtering targets were produced.
- oxidized Bi powder oxidized Bi manufactured by Mitsuwa Chemical Co., Ltd., purity 99.99%, average particle diameter 7.5 ⁇ m, standard deviation SD 1.1 ⁇ m
- Co powder manufactured by UMICORE, purity 99.9%, average particle diameter 10 ⁇ m, standard deviation SD 2.0 ⁇ m
- Ge powder manufactured by Wako Pure Chemical Industries, purity 99.99%, average particle size 11 ⁇ m, standard deviation SD 2.4 ⁇ m
- these raw material powders were put into a vibration mill and mixed under wet conditions. Specifically, after adding an alumina ball having a diameter of 10 mm, 400 g of the above raw material powder (228 g of oxidized Bi powder, 132 g of Co powder, 40 g of Ge powder) and 700 mL of water in a vibration mill, the conditions shown in Table 1 were added. Mixed. Then, after drying at 140 degreeC for 2 hours, it crushed using the mortar, and what passed the 36 mesh sieve was used for the next sintering process.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 1000 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. 7 sputtering target was manufactured.
- oxidized Sn powder oxidized Sn manufactured by Mitsuwa Chemical, purity 99.9%, average particle size 5.0 ⁇ m, standard deviation SD 1.1 ⁇ m
- Pd powder and Ag powder used in 3 were prepared.
- coarse particles were previously removed using a 100-mesh sieve, and only those that passed through the sieve were used.
- these raw material powders were put into a ball mill and mixed under wet conditions. More specifically, after adding ⁇ 10 mm alumina balls, 450 g of the above raw material powder (265 g of oxidized Sn powder, 135 g of Pd powder, 22.5 g of Ag powder) and 700 mL of water in a ball mill, the conditions shown in Table 1 were added. Mixed. Then, after drying at 140 degreeC for 2 hours, it crushed using the mortar, and what passed the 36 mesh sieve was used for the next sintering process.
- Sintering method is no. In the same manner as in No. 1, a spark plasma sintering machine was used, and sintering was performed at a heating temperature of 1000 ° C. and an applied pressure of 40 MPa for 1 hour. Next, no. 1 performs machining in the same manner as, No. 8 sputtering targets were produced.
- these raw material powders are No.
- the mixture was added to the mixer with stirring blades used in 3 and mixed. Specifically, after adding 400 g of the raw material powder (160 g of Zn oxide powder, 20 g of oxidized Co powder, 160 g of Pd powder, and 60 g of Cu powder) to the above mixer, mixing is performed under the conditions shown in Table 1. This was used for the next sintering step.
- Sintering method is no. In the same manner as in No. 1, a spark plasma sintering machine was used, and sintering was performed at a heating temperature of 900 ° C. and an applied pressure of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. 9 sputtering targets were produced.
- these raw material powders were put into a V mixer and mixed. Specifically, 400 g of the above raw material powder (188 g of oxidized Bi powder, 80 g of oxidized Ge powder, and 132 g of Pd powder) was added to the V mixer, and then mixed under the conditions shown in Table 1. Then, after drying at 140 degreeC for 2 hours, it crushed using the mortar, and what passed the 100 mesh sieve was used for the following sintering process.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 1000 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. 1 performs machining in the same manner as, No. Ten sputtering targets were manufactured.
- these raw material powders were put into a V mixer and mixed. Specifically, after adding 400 g of the above raw material powder (204 g of Zn oxide powder, 156 g of Pd powder, 40 g of Cu powder) in the V mixer, the mixture obtained under the conditions shown in Table 1 is used in the next sintering step. Used for.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 950 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. 11 sputtering targets were produced.
- these raw material powders were put into a V mixer and mixed. Specifically, after adding 400 g of the above raw material powder (228 g of oxidized In powder and 172 g of Pd powder) in a V mixer, a mixture obtained under the conditions shown in Table 1 was used in the next sintering step.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 1000 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. To produce a 12 sputtering target.
- these raw material powders were charged in a V mixer and mixed. Specifically, after adding 400 g of the raw material powder (244 g of Zn oxide powder and 156 g of Pd powder) in the V mixer, the mixture under the conditions shown in Table 1 was used for the next sintering step.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 950 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. Thirteen sputtering targets were manufactured.
- oxidized In powder (same as No. 1), Zn oxide powder (same as No. 2), oxidized Al powder (Mitsuwa Chemical Al oxide, purity 99.99%, average particle size 0.3 ⁇ m, standard) Deviation SD 0.1 ⁇ m) and Pd powder (same as No. 1) were prepared.
- these raw material powders were put into a ball mill and mixed under wet conditions. Specifically, after adding ⁇ 10 mm alumina balls, 500 g of the above raw material powder (335 g of oxidized In powder, 65 g of Zn oxide powder, 30 g of oxidized Al powder, and 70 g of Pd powder) and 700 mL of water in a ball mill, It was mixed under the conditions shown in Table 1. Then, after drying at 140 degreeC for 2 hours, it crushed using the mortar, and what passed the 36 mesh sieve was used for the next sintering process.
- Sintering method is no. In the same manner as in Example 1, using a discharge plasma sintering machine, sintering was performed at a heating temperature of 950 ° C. and a pressing force of 50 MPa for 1 hour. Next, no. Machining was performed in the same manner as in No. 1, and no. 14 sputtering targets were manufactured.
- the above sputtering target was attached to a sputtering apparatus (a sputtering system “HSR-542S” manufactured by Shimadzu Corporation), and DC magnetron sputtering was performed.
- a sputtering apparatus a sputtering system “HSR-542S” manufactured by Shimadzu Corporation
- DC magnetron sputtering was performed.
- the number of occurrences of abnormal discharge (arcing) was measured by an arc monitor (micro arc monitor “MAM Genesis” measuring instrument manufactured by Landmark Technology) connected to the power source of the sputtering apparatus.
- the conditions for DC magnetron sputtering were Ar flow rate: 10 sccm, oxygen flow rate: 10 sccm, gas pressure: 0.4 Pa, DC sputtering power: 200 W, and substrate temperature: room temperature.
- abnormal discharge was evaluated based on the following criteria. In this example, it was determined that abnormal discharge did not occur (arcing occurrence count 0) was abnormal discharge pass (A), and occurrence (arcing occurrence count 1 or more) was abnormal discharge reject (B).
- the operational stability was evaluated based on the following criteria.
- the case where the evacuation time was 2 hours or less was determined to pass the operation stability (A), and the case where the vacuuming time exceeded 2 hours was determined to be the operation stability reject (B).
- No. 1 prepared by the preferred mixing method of the present invention.
- Nos. 1 to 10 and 14 were able to prevent abnormal discharge during sputtering because the maximum equivalent circle diameter of the metal oxide was controlled to 200 ⁇ m or less regardless of the composition of the sputtering target.
- those in which the relative density was appropriately controlled Nos. 1 to 5, 7 to 9, and 14 were found to have excellent operational stability.
- No. Nos. 5, 7, and 14 are examples in which wet mixing was performed without prior sieving.
- the maximum value of the circle equivalent diameter of the metal oxide was slightly larger than 1, 2, 4, and 8, the range of the present invention was satisfied, so that abnormal discharge during sputtering could be prevented.
- the relative density was appropriately controlled, the operation stability was also good.
- No. 3 is an example of pre-sieving and then mixing with a mixer equipped with a stirring blade. Both the maximum value of the circle equivalent diameter and the relative density of the metal oxide are appropriately controlled, and abnormal discharge during sputtering is performed. In addition, the operational stability was good.
- No. Nos. 6 and 9 are examples of mixing with a mixer equipped with a stirring blade without prior sieving. Although the maximum value of the circle equivalent diameter of the metal oxide was slightly larger than that of No. 3, the range of the present invention was satisfied, so that abnormal discharge during sputtering could be prevented. In addition, No. 6, the relative density of the sputtering target is lowered.
- No. No. 10 is an example of pre-sieving and then mixing with a V mixer under a dry method.
- the maximum value of the circle equivalent diameter of the metal oxide was kept small, and no abnormal discharge occurred.
- No. Nos. 11 to 13 are examples of mixing with a V mixer under a dry method without performing sieving in advance, and the maximum value of the circle equivalent diameter of the metal oxide was increased, and abnormal discharge occurred during sputtering.
- No. 12 and 13 are No. Since the oxide content was higher than 11, the relative density of the sputtering target was lowered, and the operational stability was poor. Oxides generally have a higher melting point than metals, so oxides are more stable at the same temperature, atomic diffusion is slow, and sintering is less likely to proceed. Further, the hardness is high, and at the same temperature and pressure, the particles do not deform and the voids between the particles cannot be filled. For these reasons, the relative density decreases when the oxide content is high.
- No. 1 no. 2 (eg both the present invention), No. 12 (comparative example) micrographs are shown in FIGS. 1 (a) to 1 (b), 2 (a) to 2 (b), and 3 (a) to 3 (b), respectively.
- No. 1 and no. No. 2 does not satisfy the requirements of the present invention, while the maximum equivalent circle diameter of the metal oxide is controlled to be low.
- No. 12 had a large maximum equivalent circle diameter of the metal oxide, and a large oxide aggregate phase was observed.
- the maximum value of the equivalent circle diameter of the metal oxide is controlled to 200 ⁇ m or less, so that abnormal discharge occurs during sputtering or cracking of the sputtering target due to thermal stress occurs.
- a metal oxide-metal composite recording layer corresponding to the composition of the sputtering target can be efficiently produced without causing the problem of occurrence.
- the relative density of the metal oxide-metal composite sputtering target of the present invention is preferably controlled to 92% or more, the operation can be performed without causing problems such as generation of gas from the sputtering target during sputtering. Stable and productive.
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Abstract
Description
(1)金属酸化物Aと、金属Bとを含む金属酸化物-金属複合スパッタリングターゲットであって、前記金属酸化物Aの円相当直径の最大値が200μm以下に制御されている金属酸化物-金属複合スパッタリングターゲット。
なお、上記(1)の金属酸化物Aと、金属Bとを含む金属酸化物-金属複合スパッタリングターゲットにおいて、金属酸化物Aは凝集していても良い。
(2)相対密度が92%以上である(1)に記載の金属酸化物-金属複合スパッタリングターゲット。
(3)前記金属酸化物Aを構成する金属AMと、前記金属Bは、同一または異なっている(1)又は(2)に記載の金属酸化物-金属複合スパッタリングターゲット。
(4)前記金属酸化物Aは、酸化In、酸化Bi、酸化Zn、酸化W、酸化Sn、酸化Co、酸化Ge、および酸化Alよりなる群から選択される少なくとも一種である(1)~(3)のいずれかに記載の金属酸化物-金属複合スパッタリングターゲット。
(5)前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である(1)~(4)のいずれかに記載の金属酸化物-金属複合スパッタリングターゲット。
(6)光情報記録媒体用記録層の形成に用いられるものである(1)~(5)のいずれかに記載の金属酸化物-金属複合スパッタリングターゲット。
まず、測定対象となるスパッタリング面を用意する。ここでは、金属酸化物Aの円相当直径を測定し易いように、スパッタリングターゲットをスパッタリング面と平行する面で切断し、測定対象となるスパッタリング面を露出させる。測定対象は、スパッタリングターゲット表面近傍、好ましくはターゲット最表面の切断面を測定対象とする。
(1)混合機について
(1a)せん断作用を有する混合機の使用
混合工程に用いられる混合機は、攪拌羽根付きV型混合機、内設羽根付き水平円筒型混合機などのように、原料粉末のせん断作用を有する混合機を用いて混合することが好ましい。混合機に設置された攪拌羽根や内設羽根などにより、金属酸化物Aが凝集したとしても凝集部分(凝集相)が解砕されるため、原料粉末の凝集が抑制されるからである。
あるいは、本発明では、せん断作用を有しない通常の混合機[V型混合機(Vミキサー)、水平円筒型混合機など]を用いることもできる。この場合は、後記(2)に記載するように、金属酸化物Aについて、混合前に原料粉末(金属酸化物A)の粒度分布を適切に制御しておくことが好ましく、これにより、金属酸化物Aの円相当直径の最大値が適切に制御されたスパッタリングターゲットを得ることができる(後記する実施例を参照)。
あるいは、本発明では、ボールミルや振動ミルなどのミルを混合機として用いることもできる。ミルは通常、原料粉末を砕くのに用いられるが、本発明では、原料粉末の解砕と混合を兼ねてミルを用いることができる。ミルを用いて混合する場合は、湿式下で行なうことが好ましく、これにより、金属酸化物Aの円相当直径の最大値を、所定範囲に低く抑えることができる(後記する実施例を参照)。ここで、湿式下とは、水などの溶媒存在下で混合することを意味する。混合条件は特に限定されず、金属酸化物Aの円相当直径の最大値が200μmを超えないように、原料粉末の種類や量、ミルの種類などに応じて、適宜適切に設定すれば良い。具体的には、例えば、原料粉末とアルミナボールと水を、ボールミルに投入し、所定時間混合した後、取り出して乾燥し、好ましくは乳鉢内ですりつぶす等して粗粉砕を行い、36メッシュの篩にかけてから、焼結工程に供することが好ましい。
特に金属酸化物Aについて、混合前に粗大な粉末を除去して粒度分布を適切に制御する目的で、所定サイズの篩にかけ、篩を通ったもののみを混合することが好ましい。具体的には、金属酸化物Aについて、例えば、100メッシュ(=篩の目のサイズ150μm)の篩を用い、金属酸化物Aの円相当直径の平均値を、おおむね、150μm以下に制御しておくことが好ましい。
上記のようにして得られた混合粉末を焼結する。焼結方法としては、HIP(Hot Isostatic Pressing)、ホットプレスなどが挙げられるが、後記する実施例に記載の放電プラズマ焼結を行なうことが好ましい。放電プラズマ焼結法は、混合粉末を加圧しながら直流パルス電流を流し、粉末間で放電プラズマを発生させて焼結を行なう方法であり、短時間(数分程度)で焼結でき、取り扱いが容易であるなどの利点を有している。放電プラズマ焼結法の具体的な条件は、原料粉末の種類や量などによって相違するため、予備実験で加熱温度を決定する。また、密度を高くするためには、加圧力は高いほうがよく、おおむね、40~50MPaの範囲内に制御することが好ましい。
上記のようにして得られた焼結体を機械加工することによってスパッタリングターゲットを製造する。機械加工方法としては、旋盤やフライス盤などを用いた機械加工が挙げられるが,後記する実施例に記載のNC旋盤を用いた機械加工が好ましい。
表1に示す様々な組成の金属酸化物A-金属Bを含む複合スパッタリングターゲット(No.1~14)について、表1に記載の方法で混合した後、焼結し、機械加工を行って製造した。
原料粉末として、酸化In粉末(稀産金属製酸化In、純度99.9%、平均粒径7.3μm、標準偏差SD1.0μm)およびPd粉末(石福金属製、平均粒径2.0μm、標準偏差SD0.5μm)を用意した。
No.1において、原料粉末として、酸化In粉末の代わりに酸化Zn粉末(本庄ケミカル製酸化Zn:純度99.7%、平均粒径4.5μm、標準偏差SD1.1μm)を用い、酸化Zn粉末とPd粉末の混合量を、酸化Zn粉末:244g、Pd粉末:156 gとしたこと以外は、No.1と同様にして、No.2のスパッタリングターゲットを製造した。
原料粉末として、No.1に用いた酸化In粉末およびPd粉末のほかに、更にAg粉末(徳力化学製、純度99.9%、平均粒径10μm、標準偏差SD1.0μm)を用意した。このうち酸化In粉末は、No.1と同様、予め、100メッシュの篩を用いて粗大なものを除去し、篩を通過したもののみを用いた。
原料粉末として、No.1に用いた酸化In粉末およびPd粉末のほかに、更にW粉末(和光純薬製、純度99.9%、平均粒径3.5μm、標準偏差SD0.8μm)を用意した。このうち酸化In粉末は、No.1と同様、予め、100メッシュの篩を用いて粗大なものを除去し、篩を通過したもののみを用いた。
原料粉末として、酸化Zn粉末(No.2と同じ)、酸化W粉末(和光純薬製酸化W、純度99.9%、平均粒径6.5μm、標準偏差SD1.4μm)、およびNo.1に用いたPd粉末を用意した。
原料粉末として、No.1に用いた酸化In粉末およびPd粉末を用意した。
原料粉末として、酸化Bi粉末(三津和化学製酸化Bi、純度99.99%、平均粒径7.5μm、標準偏差SD1.1μm)、Co粉末(UMICORE製、純度99.9%、平均粒径10μm、標準偏差SD2.0μm)、およびGe粉末(和光純薬製、純度99.99%、平均粒径11μm、標準偏差SD2.4μm)を用意した。
原料粉末として、酸化Sn粉末(三津和化学製酸化Sn、純度99.9%、平均粒径5.0μm、標準偏差SD1.1μm)、並びにNo.3に用いたPd粉末およびAg粉末を用意した。このうち酸化Sn粉末は、予め、100メッシュの篩を用いて粗大なものを除去し、篩を通過したもののみを用いた。
原料粉末として、No.5に用いた酸化Zn粉末と、酸化Co粉末(三津和化学製酸化Co、純度99.9%、平均粒径6.3μm、標準偏差SD1.3μm)と、No.1に用いたPd粉末と、Cu粉末(山石金属製、純度99.9%、平均粒径12μm、標準偏差SD2.3μm)を用意した。
原料粉末として、No.7に用いた酸化Bi粉末と、酸化Ge粉末(稀産金属製酸化Ge、純度99.99%、平均粒径7μm、標準偏差SD1.0μm)と、No.1に用いたPd粉末を用意した。このうち酸化Bi粉末および酸化Ge粉末は、予め、100メッシュの篩を用いて粗大なものを除去し、篩を通過したもののみを用いた。
原料粉末として、No.2に用いた酸化Zn粉末と、No.1に用いたPd粉末、No.9に用いたCu粉末を用意した。
原料粉末として、No.1に用いた酸化In粉末と、No.1に用いたPd粉末を用意した。
原料粉末として、No.2に用いた酸化Zn粉末と、No.1に用いたPd粉末を用意した。
原料粉末として、酸化In粉末(No.1と同じ)、酸化Zn粉末(No.2と同じ)、酸化Al粉末(三津和化学酸化Al、純度99.99%、平均粒径0.3μm、標準偏差SD0.1μm)およびPd粉末(No.1と同じ)を用意した。
上記のスパッタリングターゲットをスパッタリング装置(島津製作所製のスパッタリングシステム「HSR-542S」)に取り付け、DCマグネトロンスパッタリングを行なった。このとき、スパッタリング装置の電源に接続したアークモニター(ランドマークテクノロジー製のマイクロアークモニター「MAM Genesis」計測器)によって異常放電(アーキング)の発生回数を測定した。なお、DCマグネトロンスパッタリングの条件は、Ar流量:10sccm、酸素流量:10sccm、ガス圧:0.4Pa、DCスパッタリングパワー:200W、基板温度:室温とした。
また、上記のスパッタリングターゲットをスパッタリング装置(島津製作所製のスパッタリングシステム「HSR-542S」)に取り付け、DCマグネトロンスパッタリングを行なうにあたり、スパッタリングチャンバーを背圧0.27×10-3Paまで真空引きを行なう。相対密度が低い場合は、スパッタリングターゲット中の気孔に存在するガスが放出され、この真空引きに長い時間を要する。そこで、所定の背圧に達するまでの真空引き時間を測定した。
本出願は、2009年9月18日出願の日本特許出願(特願2009-217750)、2010年2月10日出願の日本特許出願(特願2010-028094)に基づくものであり、その内容はここに参照として取り込まれる。
Claims (17)
- 金属酸化物Aと、金属Bとを含む金属酸化物-金属複合スパッタリングターゲットであって、前記金属酸化物Aの円相当直径の最大値が200μm以下に制御されている金属酸化物-金属複合スパッタリングターゲット。
- 相対密度が92%以上である請求項1に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属酸化物Aを構成する金属AMと、前記金属Bは、同一または異なっている請求項1に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属酸化物Aを構成する金属AMと、前記金属Bは、同一または異なっている請求項2に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属酸化物Aは、酸化In、酸化Bi、酸化Zn、酸化W、酸化Sn、酸化Co、酸化Ge、および酸化Alよりなる群から選択される少なくとも一種である請求項1に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属酸化物Aは、酸化In、酸化Bi、酸化Zn、酸化W、酸化Sn、酸化Co、酸化Ge、および酸化Alよりなる群から選択される少なくとも一種である請求項2に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属酸化物Aは、酸化In、酸化Bi、酸化Zn、酸化W、酸化Sn、酸化Co、酸化Ge、および酸化Alよりなる群から選択される少なくとも一種である請求項3に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属酸化物Aは、酸化In、酸化Bi、酸化Zn、酸化W、酸化Sn、酸化Co、酸化Ge、および酸化Alよりなる群から選択される少なくとも一種である請求項4に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項1に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項2に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項3に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項4に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項5に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項6に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項7に記載の金属酸化物-金属複合スパッタリングターゲット。
- 前記金属Bは、Pd、Ag、W、Cu、Ge、Co、およびAlよりなる群から選択される少なくとも一種である請求項8に記載の金属酸化物-金属複合スパッタリングターゲット。
- 光情報記録媒体用記録層の形成に用いられるものである請求項1~16のいずれか一項に記載の金属酸化物-金属複合スパッタリングターゲット。
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JP5399836B2 (ja) * | 2009-09-18 | 2014-01-29 | 株式会社神戸製鋼所 | 光情報記録媒体用記録層、光情報記録媒体およびスパッタリングターゲット |
JP5399184B2 (ja) * | 2009-09-18 | 2014-01-29 | 株式会社神戸製鋼所 | 光情報記録媒体およびスパッタリングターゲット |
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Also Published As
Publication number | Publication date |
---|---|
US20120181172A1 (en) | 2012-07-19 |
EP2479312A4 (en) | 2015-06-17 |
JP2011084804A (ja) | 2011-04-28 |
EP2479312B1 (en) | 2017-01-25 |
CN102498233A (zh) | 2012-06-13 |
EP2479312A1 (en) | 2012-07-25 |
TW201125999A (en) | 2011-08-01 |
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